In order to improve the electrochemical performance of polyoxomolybdate Na3[AlMo6O24H6]（NAM） as the cathode material of lithium ion battery, the NAM materials with small particle size were synthesized by elevatingth...In order to improve the electrochemical performance of polyoxomolybdate Na3[AlMo6O24H6]（NAM） as the cathode material of lithium ion battery, the NAM materials with small particle size were synthesized by elevatingthe synthesistemperaturein the solution.The as-prepared NAM materials were investigated by FT-IR, XRD, SEM and EIS. Their discharge-charge and cycle performance were also tested. The resultsshowthat the particle size decreasesto less than10μm at the temperature ofhigher than 40℃.When synthesized at 80℃,the NAMwiththe smallest particle size （-3μm）exhibitsthe best electrochemical performance such ashigh initial discharge capacity of 409 mA·h/gandcoulombic efficiency of 95% in the first cycle at 0.04C.展开更多
A new polyoxomolybdate compound,namely {[MnII（L）（4,4？-Hbipy）（H2O）2]2 [Mo5O15（PO4）2]}.2H2O 1（L = 3-（2-pyridyl）pyrazole,4,4＇-Hbipy = protonated 4,4＇-bipyridine）,was designed and synthesized under hydrothe...A new polyoxomolybdate compound,namely {[MnII（L）（4,4？-Hbipy）（H2O）2]2 [Mo5O15（PO4）2]}.2H2O 1（L = 3-（2-pyridyl）pyrazole,4,4＇-Hbipy = protonated 4,4＇-bipyridine）,was designed and synthesized under hydrothermal conditions.Single-crystal X-ray diffraction analysis result reveals that the [Mo5O15（PO4）2]6-cluster in compound 1 links to two MnII cations via the oxygen of PO43-,which is further coordinated by one 3-（2-pyridyl）pyrazole,one 4,4＇-Hbipyridine,and two water molecules.展开更多
The polyoxometalate（POM）-imidazole ionic liquid（IL） [C8mim]2[Mo6O19]（C8mim=1-methyl-3-octylimi- dazolium） with a low melting point of 82.6 °C was successfully prepared and characterized by FTIR, XPS, NMR, T...The polyoxometalate（POM）-imidazole ionic liquid（IL） [C8mim]2[Mo6O19]（C8mim=1-methyl-3-octylimi- dazolium） with a low melting point of 82.6 °C was successfully prepared and characterized by FTIR, XPS, NMR, TG and so on. The polyoxomolybdate-based IL has high stability, and its decomposing temperature reaches 321 °C, which is higher than that of 1-alkyl-3-methylimidazolium halides IL. Further photocatalytic performances of the IL were measured via degrading dye rhodamine B（RB） in aqueous solution under the UV light irradiation. The experiments show that the conversion of RB reaches 80.5% after 90 min under UV-light and the degradation efficiency depends on the pH value of the solution, irradiation time and the dosage of the IL and so on.展开更多
The title compound, [{Na（H2O）3}2lRu（dmso）3}2（MoO4）3]·3H2O, has been obtained by the reaction of Na2MoO4·2H2O with cis-Ru（dmso）4Cl2 in aqueous solution. Its crystal structure was determined by single-...The title compound, [{Na（H2O）3}2lRu（dmso）3}2（MoO4）3]·3H2O, has been obtained by the reaction of Na2MoO4·2H2O with cis-Ru（dmso）4Cl2 in aqueous solution. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the triclinic system, space group PI^- with a = 12.3333（3）, b = 12.6289（3）, c = 32.0284（14） A, α = 79.873（7）, β= 87.549（9）, γ = 64.500（4）°, V = 4429.5（2） A^3, Z = 4, Mr = 1358.85, Dc = 2.038 g/cm^3, F（000） = 2696 and μ = 1.874 mm^-1. The compound contains a novel pentanuclear triangle bipyramidal core, [{ Ru（dmso）3 } 2（MoO4）3]^2-, which consists of two { Ru（dmso）3 } ^2＋ fragments and three {μ2-MoO4}^2- units. Furthermore, the dmso ligands bridge the pentanuclear [Ru2Mo3] core and two [Na（H2O）3]^＋ fragments together, forming a neutral heptanuclear ruthenium- and sodiumcontaining polyoxomolybdate.展开更多
The polyoxoanion incorporated {Mn（CO）3^＋} complex, （n-Bu4N）2[Mo6O16（OCH3）2{HOCH2C（CH2O）3}2·{Mn（CO）3}2]（1）, has been synthesized by the reaction of （n-Bu4N）4[Mo8O26] with Mn（CO）5Br in methanol, in...The polyoxoanion incorporated {Mn（CO）3^＋} complex, （n-Bu4N）2[Mo6O16（OCH3）2{HOCH2C（CH2O）3}2·{Mn（CO）3}2]（1）, has been synthesized by the reaction of （n-Bu4N）4[Mo8O26] with Mn（CO）5Br in methanol, in the presence of C（CH2OH）4. The complex 1 has been characterized by IR, UV-Vis, X-ray single crystal diffraction, and TG. Crystal data for the complex 1：C25H48MnMo3NO16 （1）, Triclinic Pi, a=0.9405（3） nm, b=1.3351（4） nm, c=1.5455（4） nm, α=103.206（5）°, β=102.165（5）°, γ=100.784（5）°, V=1.7896（9） nm^3, Z=2, R1=0.0703, wR2= 0.1495. The structure analysis of complex 1 shows that the complex consists of two tetrabutylammonium cations and a polyoxomolybdate anion that incorporates two fac-Mn（CO）3^＋ units. The anion of complex 1 can be considered as the dimer of two rhomb-like anions by sharing of two comers.展开更多
A new polyoxomolybdate complex HNaT[Mo36O112（H2O）16]·47H2O 1 has been prepared in the beaker solution and characterized by single-crystal X-ray diffraction and elemental analyses. Crystal data： H127Mo36Na7O175...A new polyoxomolybdate complex HNaT[Mo36O112（H2O）16]·47H2O 1 has been prepared in the beaker solution and characterized by single-crystal X-ray diffraction and elemental analyses. Crystal data： H127Mo36Na7O175, Mr = 6542.79, monoclinic, C2/c, a = 40.891（6）, b = 17.900（3）, c = 25.580（4）A, β = 125.673（2）°, V = 15210（4）A3, Z = 4, Dc = 2.857 g/cm^3, F（000） = 12464,μ = 3.013 mm^-1, R = 0.0633 and wR = 0.1654 （I 〉 20（I））. With the bridging sodium cations, the [Mo36Ou2（H2O）16]^8- units in compound 1 are linked to form a one-dimensional structure, on the basis of which a three-dimensional architecture is further constructed via other sodium cations and complicated hydrogen bonds.展开更多
In this paper,One novel Keggin type polyoxomolybdate compounds have been hydrothermal synthesized:{[(CH3)2NH2]4(SiMo12O40)}[(CH3)2NH]·(DMF)0.5(1).The compound 1have been characterized by infrared spectrum,and the...In this paper,One novel Keggin type polyoxomolybdate compounds have been hydrothermal synthesized:{[(CH3)2NH2]4(SiMo12O40)}[(CH3)2NH]·(DMF)0.5(1).The compound 1have been characterized by infrared spectrum,and the two-dimensional infrared correlation spectroscopy.展开更多
Two new polyoxomolybdate compounds,namely CuII2（HL）3]2[Mo8O26]·（H2O）4（1） and [NiII（HL）3]2（Mo8O26）·（H2O）3（2）（HL = 3-（2-pyridyl）pyrazole）,were designed and synthesized under hydrothermal cond...Two new polyoxomolybdate compounds,namely CuII2（HL）3]2[Mo8O26]·（H2O）4（1） and [NiII（HL）3]2（Mo8O26）·（H2O）3（2）（HL = 3-（2-pyridyl）pyrazole）,were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu（II） ions linked by three 3-（2-pyridyl）pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-（2-pyridyl）pyrazole ligands.Crystal data of 1：C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850（2）,b = 18.510（4）,c = 17.230（3） ,β = 100.57（3）°,V = 3401.6（12） 3,Z = 4,Dc = 2.324 g/cm3,F（000） = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775（Ⅰ 〉 2σ（Ⅰ））;Crystal data for 2：C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799（2）,b = 14.7970（13）,c = 23.141（2） ,β = 91.6180（10）°,V = 7119.0（11） 3,Z = 4,Dc = 2.077 g/cm3,F（000） = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696（Ⅰ〉 2σ（Ⅰ））.展开更多
Polyoxomolybdate [Mo36O110（NO）4（H2O）14].52H2O was synthesized by a simple one-pot procedure through reducing an acidified mixture of Na2MoO4.2H2O and NH2OH. HCl. In order to create a heterogeneous catalyst system,...Polyoxomolybdate [Mo36O110（NO）4（H2O）14].52H2O was synthesized by a simple one-pot procedure through reducing an acidified mixture of Na2MoO4.2H2O and NH2OH. HCl. In order to create a heterogeneous catalyst system, the polyoxomolybdate was pillared with MgAI-LDH-NO3 by direct ion exchange. These novel materials were carefully analyzed by various chemico-physical methods, The catalytic degradation of methylene blue （MB） and rhodamine B （RB） as common dyes in the presence of MgAl-LDH-1 nanoparticles with aqueous hydrogen peroxide, H2O2, as an oxidizing agent was studied in aqueous solution at room temperature. More importantly, the catalyst can be recovered and reused efficiently up to five consecutive cycles with negligible loss of catalytic activity.展开更多
Highly reduced molybdenum red(MR)clusters have emerged as a new type of polyoxomolybdates(POMos)and showed great potential as electron/proton reservoirs for energy conversion and storage,as well as for catalysis.Howev...Highly reduced molybdenum red(MR)clusters have emerged as a new type of polyoxomolybdates(POMos)and showed great potential as electron/proton reservoirs for energy conversion and storage,as well as for catalysis.However,the limited structural diversity of MR clusters significantly hinders further exploration of their potential as functional materials.Herein,we describe the synthesis of a novel highly reduced MR cluster{Mo_(49)}(compound 1)based on rational assembly of a variety of basic building blocks(BBs).In addition to the well-established BBs found in the family of MR clusters,the unique tetrahedral{MoVI 4}BB plays a key role in directing the assembly to afford trigonal pyramid-like structure of compound 1,which consists of 49 Mo and 148 O atoms with a high reduction degree of 73%.Moreover,at 80℃and 98%relative humidity(RH),the pellet sample of compound 1 displays good proton conductivity of 7.88×10^(-3)S/cm owing to the efficient hydrogen-bonded network built from the surface oxygen atoms,protons and vip water molecules.This research offers new insights into the assembly and synthesis of MR clusters through a BB strategy and manifests their significant potential for advanced applications.展开更多
Ce/Sm ions are covalently grafted to a Keggin polyoxomolybdate cluster[PMo12O40]3-to yield interesting fluorescent-photodarkening molecular systems.Their photoresponce processes are observed to be activated via energy...Ce/Sm ions are covalently grafted to a Keggin polyoxomolybdate cluster[PMo12O40]3-to yield interesting fluorescent-photodarkening molecular systems.Their photoresponce processes are observed to be activated via energy transfer from luminescent fragments to photocoloration components.展开更多
Three polyoxomolybdate compounds,namely {[MII(HL)2]2(Mo8O26)}n(M = Co(1),Ni(2),Zn(3))(HL,3-(2-pyridyl)pyrazole),were designed and synthesized under the hydrothermal conditions and characterized by elemental analysis,I...Three polyoxomolybdate compounds,namely {[MII(HL)2]2(Mo8O26)}n(M = Co(1),Ni(2),Zn(3))(HL,3-(2-pyridyl)pyrazole),were designed and synthesized under the hydrothermal conditions and characterized by elemental analysis,IR spectroscopy,and TGA.Single-crystal X-ray diffraction analysis results reveal that compounds 1-3 own the isostructural chain structure consisting of the β-[Mo8O26]4- anions,which are linked by M(HL)22+ units via the terminal oxygen atoms.TGA curves show that the organic ligands separate from the related compounds above ca.673 K.展开更多
Since two interesting inorganic “host vip” polyoxomolybdates 1 and 2 have been reported previously, we have now succeeded in selectively isolating three new acetated “host vip” polyoxomolybdates 3—5, which ...Since two interesting inorganic “host vip” polyoxomolybdates 1 and 2 have been reported previously, we have now succeeded in selectively isolating three new acetated “host vip” polyoxomolybdates 3—5, which considerably extend the range of structures in the cyclic polyoxomolybdate catalogue. 3 crystallizes in the triclinic space group P 1 with a =1 22235(1) nm, b =1 52977(2) nm, c =1 54022(1) nm, α =113 746(1)°, β =96 742(1)°, γ = 101 564(1)°, V =2 51892(4) nm 3, Z =1, D c=2 568 g·cm -3 . 4 and 5 crystallize in the monoclinic system: P 2(1)/ n , a =1 08298(2) nm, b =1 54029(1) nm, c = 2 78893(5) nm, β =94 2730(10)°, V =4 63929(12) nm 3, Z =2 and D c=2 671 g·cm -3 for 4, and C 2/ c , a =2 59907(8) nm, b =1 65992(3) nm, c =2 28473(7) nm, β = 93 4370(10)° , V =9 8392(5) nm 3, Z =4 and D c=2 556 g·cm -3 for 5. The structures of 3, 4 and 5 consist of 18 membered “host vip” polyoxoanions [{Na(X) 2}{( μ 3 OH) 4Mo V 8Mo VI 10 O 52 ( μ 2 CH 3COO) 2}] -( n +9) (X=CH 3COO - for 3, DMF for 4 and H 2O for 5), which are connected via Na + ions or hydrogen bonds into infinite extended frameworks.展开更多
A new polyoxomolybdate compound [Ag 3 （HL） 4 ]（PMo 12 O 40）] 1 （HL=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analys...A new polyoxomolybdate compound [Ag 3 （HL） 4 ]（PMo 12 O 40）] 1 （HL=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375（3）,b=12.076（3）,c=13.196（4）,α=84.170（4）,β=71.961（3）,γ=86.326（4）°,V=1563.1（7）3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ（MoKα）=3.366 mm 1,F（000）=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections （I 2σ（Ⅰ））.X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 （HL） 4 3＋ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 （HL） 4 3＋ exhibits two distinct Ag（Ⅰ） environments：a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.展开更多
A new polyoxomolybdate compound [Zn（HL）2（Mo8O26）（4,4＇-Bipy）]·（4,4＇-Bipy） （HL = 3-（2-pyridyl）pyrazole, 4,4＇-Bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characteri...A new polyoxomolybdate compound [Zn（HL）2（Mo8O26）（4,4＇-Bipy）]·（4,4＇-Bipy） （HL = 3-（2-pyridyl）pyrazole, 4,4＇-Bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, TG and IR spectroscopy. The compound crystallizes in monoclinic, space group C2/c with a = 18.060（4）, b = 13.870（3）, c = 19.360（4） A, β = 93.50（3）°, V = 4840.5（17） 3, C36H30Mo8N10O26Zn, Mr = 1851.59, Dc = 2.541 g/cm^3, μ（MoKα） = 2.589 mm·1, F（000） = 3560, Z = 4, the final R = 0.0328 and wR = 0.0870 for 4005 observed reflections （I 〉 2σ（I））. X-ray diffraction analyses reveal that compound 1 is constructed from Mo8O264-units linked by Zn（HL）22＋ and 4,4＇-Bipy. Mo8O264-is connected by Zn（HL）2^2＋ via terminal oxygen atoms along the [010] axis forming chains, which are further linked by 4,4＇-Bipy along the [001] axis forming a two-dimensional network structure.展开更多
The title compound, {(H3O)4(NH4)4[Mo8O28]?2H2O}n 1, has been synthesized from the reaction of Zn(OAc)2 and (NH4)6Mo7O24?4H2O in aqueous solution at ambient tempe- rature, and its crystal structure was determined by ...The title compound, {(H3O)4(NH4)4[Mo8O28]?2H2O}n 1, has been synthesized from the reaction of Zn(OAc)2 and (NH4)6Mo7O24?4H2O in aqueous solution at ambient tempe- rature, and its crystal structure was determined by X-ray single-crystal analysis with the following crystallographic data: monoclinic system, space group P21/n, a = 9.5234(6), b = 11.3235(8), c = 14.8812(10) ?, β = 107.467(2)o, V = 1530.77(18) ?3, Z = 4, F(000) = 1336, μ = 3.293 mm-1 and Dc = 3.037 g/cm3. The final R = 0.0619 for 2691 observed reflections (I > 2σ(I)). X-ray crys- tal structure analysis showed that the novel one-dimensional chain compound is built up by basic {Mo8O28} units via single μ2-O, and such chains are further linked into a three-dimensional net- work by hydrogen bonds.展开更多
Polymeric systems have played an important role as structure-directing agents and in the control of nucleation and growth of crystals.This article reviews the work of our research group in the field of the polymer-ass...Polymeric systems have played an important role as structure-directing agents and in the control of nucleation and growth of crystals.This article reviews the work of our research group in the field of the polymer-assisted crystallization of inorganic materials,mainly focused on the formation of highly ordered,porous molybdenum oxide nanostructures.Different experimental parameters including the influence of poly(ethylene oxide)-containing polymers on the morphology and structure of the products obtained fr...展开更多
One new polyoxometalate compound connected via nickel/potassium cations, H8K{[Ni（H2O）5]2（H2Mo1.80W10.20O42）}Cl3·16H2O 1, was prepared and characterized by elemental analysis and IR spectroscopy. Single-crysta...One new polyoxometalate compound connected via nickel/potassium cations, H8K{[Ni（H2O）5]2（H2Mo1.80W10.20O42）}Cl3·16H2O 1, was prepared and characterized by elemental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis results reveal that clusters of [Ni（H2O）5]2（H2Mo1.80W10.20O42）}^6-in compound 1 are linked by potassium cations to form one- dimiensional chains, based on which a three-dimensional network is further constructed via the hydrogen bonds of O…O and O…Cl. Magnetic measurements show that compound 1 has paramagnetic properties. Crystal data： H62Cl3KMo1.80Ni2O68W10.20, Mr = 3461.33, monoclinic, space group C2/c, a = 18.9291（19）, b = 16.6758（17）, c = 19.1064（19）A, β = 106.6880（10）°, V = 5777.1（10）A^3, Z = 4, Dc = 3.980 g/cm^3, F（000） = 6250, μ = 21.574 mm^-1, R = 0.0579 and wR = 0.1623 （Ⅰ 〉 2σ（Ⅰ））.展开更多
A novel 3-D inorganic bimetallic compound Ag2Mo2O7 has been hydrothermally synthesized and structurally characterized by X-ray diffraction. The compound crystallizes in monoclinic, space group P21/c with a = 6.1274（3...A novel 3-D inorganic bimetallic compound Ag2Mo2O7 has been hydrothermally synthesized and structurally characterized by X-ray diffraction. The compound crystallizes in monoclinic, space group P21/c with a = 6.1274（3）, b = 13.1836（6）, c = 7.8780（3）A, β= 110.673（3）°, V = 595.42（5）A3, Z= 4, Mr= 519.62, Dc = 5.797g/cm^3, F（000） = 936,μ（MoKα） = 10.579 mm^-1, F（000） = 936, the final R = 0.0204 and wR = 0.0477 for 1268 observed reflections with I〉 2σ（I）. In the title compound, the [Mo4O16]n^8n-chains are linked through O-Ag-O bridging bonds to form a 3D network. It represents an unprecedented linking mode between the isopolyoxomolybdate chain and the transition metal oxide cluster. IR, TGA and fluorescence properties of the title compound are also studied.展开更多
文摘In order to improve the electrochemical performance of polyoxomolybdate Na3[AlMo6O24H6]（NAM） as the cathode material of lithium ion battery, the NAM materials with small particle size were synthesized by elevatingthe synthesistemperaturein the solution.The as-prepared NAM materials were investigated by FT-IR, XRD, SEM and EIS. Their discharge-charge and cycle performance were also tested. The resultsshowthat the particle size decreasesto less than10μm at the temperature ofhigher than 40℃.When synthesized at 80℃,the NAMwiththe smallest particle size （-3μm）exhibitsthe best electrochemical performance such ashigh initial discharge capacity of 409 mA·h/gandcoulombic efficiency of 95% in the first cycle at 0.04C.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No.2009.272)
文摘A new polyoxomolybdate compound,namely {[MnII（L）（4,4？-Hbipy）（H2O）2]2 [Mo5O15（PO4）2]}.2H2O 1（L = 3-（2-pyridyl）pyrazole,4,4＇-Hbipy = protonated 4,4＇-bipyridine）,was designed and synthesized under hydrothermal conditions.Single-crystal X-ray diffraction analysis result reveals that the [Mo5O15（PO4）2]6-cluster in compound 1 links to two MnII cations via the oxygen of PO43-,which is further coordinated by one 3-（2-pyridyl）pyrazole,one 4,4＇-Hbipyridine,and two water molecules.
基金Supported by the National Natural Science Foundation of China(Nos.2067101120731002+3 种基金20801004 10876002 20801005)the Specialized Research Fund for the Doctoral Program of Higher Education of China(No.200800070015).
文摘The polyoxometalate（POM）-imidazole ionic liquid（IL） [C8mim]2[Mo6O19]（C8mim=1-methyl-3-octylimi- dazolium） with a low melting point of 82.6 °C was successfully prepared and characterized by FTIR, XPS, NMR, TG and so on. The polyoxomolybdate-based IL has high stability, and its decomposing temperature reaches 321 °C, which is higher than that of 1-alkyl-3-methylimidazolium halides IL. Further photocatalytic performances of the IL were measured via degrading dye rhodamine B（RB） in aqueous solution under the UV light irradiation. The experiments show that the conversion of RB reaches 80.5% after 90 min under UV-light and the degradation efficiency depends on the pH value of the solution, irradiation time and the dosage of the IL and so on.
基金This work was supported by the State Key Laboratory of Structural Chemistry, the National Ministry of Science and Technology of China(001CB1089), the NNSFC (20273073, 20333070 and 90206040) and NSF of Fujian Province (2003J042, 2004J041 and 2004HZ01-1)
文摘The title compound, [{Na（H2O）3}2lRu（dmso）3}2（MoO4）3]·3H2O, has been obtained by the reaction of Na2MoO4·2H2O with cis-Ru（dmso）4Cl2 in aqueous solution. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the triclinic system, space group PI^- with a = 12.3333（3）, b = 12.6289（3）, c = 32.0284（14） A, α = 79.873（7）, β= 87.549（9）, γ = 64.500（4）°, V = 4429.5（2） A^3, Z = 4, Mr = 1358.85, Dc = 2.038 g/cm^3, F（000） = 2696 and μ = 1.874 mm^-1. The compound contains a novel pentanuclear triangle bipyramidal core, [{ Ru（dmso）3 } 2（MoO4）3]^2-, which consists of two { Ru（dmso）3 } ^2＋ fragments and three {μ2-MoO4}^2- units. Furthermore, the dmso ligands bridge the pentanuclear [Ru2Mo3] core and two [Na（H2O）3]^＋ fragments together, forming a neutral heptanuclear ruthenium- and sodiumcontaining polyoxomolybdate.
基金Supported by the National Natural Science Foundation of China(No.20771034)Program for New Century Excellent Talents in University of Henan Province,China(No.005HANCET-02)the Natural Science Foundation of Henan Province, China (No.0611020200)
文摘The polyoxoanion incorporated {Mn（CO）3^＋} complex, （n-Bu4N）2[Mo6O16（OCH3）2{HOCH2C（CH2O）3}2·{Mn（CO）3}2]（1）, has been synthesized by the reaction of （n-Bu4N）4[Mo8O26] with Mn（CO）5Br in methanol, in the presence of C（CH2OH）4. The complex 1 has been characterized by IR, UV-Vis, X-ray single crystal diffraction, and TG. Crystal data for the complex 1：C25H48MnMo3NO16 （1）, Triclinic Pi, a=0.9405（3） nm, b=1.3351（4） nm, c=1.5455（4） nm, α=103.206（5）°, β=102.165（5）°, γ=100.784（5）°, V=1.7896（9） nm^3, Z=2, R1=0.0703, wR2= 0.1495. The structure analysis of complex 1 shows that the complex consists of two tetrabutylammonium cations and a polyoxomolybdate anion that incorporates two fac-Mn（CO）3^＋ units. The anion of complex 1 can be considered as the dimer of two rhomb-like anions by sharing of two comers.
基金The work was supported by NNSFC (No. 20501011) Liaocheng University (31801)
文摘A new polyoxomolybdate complex HNaT[Mo36O112（H2O）16]·47H2O 1 has been prepared in the beaker solution and characterized by single-crystal X-ray diffraction and elemental analyses. Crystal data： H127Mo36Na7O175, Mr = 6542.79, monoclinic, C2/c, a = 40.891（6）, b = 17.900（3）, c = 25.580（4）A, β = 125.673（2）°, V = 15210（4）A3, Z = 4, Dc = 2.857 g/cm^3, F（000） = 12464,μ = 3.013 mm^-1, R = 0.0633 and wR = 0.1654 （I 〉 20（I））. With the bridging sodium cations, the [Mo36Ou2（H2O）16]^8- units in compound 1 are linked to form a one-dimensional structure, on the basis of which a three-dimensional architecture is further constructed via other sodium cations and complicated hydrogen bonds.
基金the NNSFC(21473030,1371033)Fujian Provincial Natural ScienceFoundation(2013J01042)the Open Fund of State Key Laboratory of Structural Chemistry(20130015)
文摘In this paper,One novel Keggin type polyoxomolybdate compounds have been hydrothermal synthesized:{[(CH3)2NH2]4(SiMo12O40)}[(CH3)2NH]·(DMF)0.5(1).The compound 1have been characterized by infrared spectrum,and the two-dimensional infrared correlation spectroscopy.
基金Supported by the 973 Key Program of the MOST (2006CB932904,2007CB815304)the National Natural Science Foundation of China (20873150,20821061,and 50772113)+2 种基金the Chinese Academy of Sciences (KJCX2-YW-M05)the Chinese Academy of Sciences (''Hundred Talents Program'') Ministry of Science and Technology of China (Project of ''973'' plan,No. 2007CB607606),and Shandong Provincial Education Department and Qilu Normal University
文摘Two new polyoxomolybdate compounds,namely CuII2（HL）3]2[Mo8O26]·（H2O）4（1） and [NiII（HL）3]2（Mo8O26）·（H2O）3（2）（HL = 3-（2-pyridyl）pyrazole）,were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu（II） ions linked by three 3-（2-pyridyl）pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-（2-pyridyl）pyrazole ligands.Crystal data of 1：C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850（2）,b = 18.510（4）,c = 17.230（3） ,β = 100.57（3）°,V = 3401.6（12） 3,Z = 4,Dc = 2.324 g/cm3,F（000） = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775（Ⅰ 〉 2σ（Ⅰ））;Crystal data for 2：C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799（2）,b = 14.7970（13）,c = 23.141（2） ,β = 91.6180（10）°,V = 7119.0（11） 3,Z = 4,Dc = 2.077 g/cm3,F（000） = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696（Ⅰ〉 2σ（Ⅰ））.
基金Supported by the Iranian National Science Foundation(INSF)and University of Maragheh
文摘Polyoxomolybdate [Mo36O110（NO）4（H2O）14].52H2O was synthesized by a simple one-pot procedure through reducing an acidified mixture of Na2MoO4.2H2O and NH2OH. HCl. In order to create a heterogeneous catalyst system, the polyoxomolybdate was pillared with MgAI-LDH-NO3 by direct ion exchange. These novel materials were carefully analyzed by various chemico-physical methods, The catalytic degradation of methylene blue （MB） and rhodamine B （RB） as common dyes in the presence of MgAl-LDH-1 nanoparticles with aqueous hydrogen peroxide, H2O2, as an oxidizing agent was studied in aqueous solution at room temperature. More importantly, the catalyst can be recovered and reused efficiently up to five consecutive cycles with negligible loss of catalytic activity.
基金National Natural Science Foundation of China(Nos.92161111 and 21901038)Program for Professor of Special Appointment(Eastern Scholar)at Shanghai Institutions of Higher Learning,ChinaInternational Cooperation Fund of Science and Technology Commission of Shanghai Municipality,China(No.21130750100)。
文摘Highly reduced molybdenum red(MR)clusters have emerged as a new type of polyoxomolybdates(POMos)and showed great potential as electron/proton reservoirs for energy conversion and storage,as well as for catalysis.However,the limited structural diversity of MR clusters significantly hinders further exploration of their potential as functional materials.Herein,we describe the synthesis of a novel highly reduced MR cluster{Mo_(49)}(compound 1)based on rational assembly of a variety of basic building blocks(BBs).In addition to the well-established BBs found in the family of MR clusters,the unique tetrahedral{MoVI 4}BB plays a key role in directing the assembly to afford trigonal pyramid-like structure of compound 1,which consists of 49 Mo and 148 O atoms with a high reduction degree of 73%.Moreover,at 80℃and 98%relative humidity(RH),the pellet sample of compound 1 displays good proton conductivity of 7.88×10^(-3)S/cm owing to the efficient hydrogen-bonded network built from the surface oxygen atoms,protons and vip water molecules.This research offers new insights into the assembly and synthesis of MR clusters through a BB strategy and manifests their significant potential for advanced applications.
基金supported by the National Natural Science Foundation of China(50971063)the Natural Science Foundation of Fujian Province of China(2003F006,2010J01042)the Scientific Research Foundation for Returned Overseas Chinese Scholars of the State Education Ministry of China
文摘Ce/Sm ions are covalently grafted to a Keggin polyoxomolybdate cluster[PMo12O40]3-to yield interesting fluorescent-photodarkening molecular systems.Their photoresponce processes are observed to be activated via energy transfer from luminescent fragments to photocoloration components.
基金supported by the Chinese Academy of Sciences ("Hundred Talents Program")Ministry of Science and Technology of China (2007CB607606)Shandong Provincial Education Department and Qilu Normal University
文摘Three polyoxomolybdate compounds,namely {[MII(HL)2]2(Mo8O26)}n(M = Co(1),Ni(2),Zn(3))(HL,3-(2-pyridyl)pyrazole),were designed and synthesized under the hydrothermal conditions and characterized by elemental analysis,IR spectroscopy,and TGA.Single-crystal X-ray diffraction analysis results reveal that compounds 1-3 own the isostructural chain structure consisting of the β-[Mo8O26]4- anions,which are linked by M(HL)22+ units via the terminal oxygen atoms.TGA curves show that the organic ligands separate from the related compounds above ca.673 K.
文摘Since two interesting inorganic “host vip” polyoxomolybdates 1 and 2 have been reported previously, we have now succeeded in selectively isolating three new acetated “host vip” polyoxomolybdates 3—5, which considerably extend the range of structures in the cyclic polyoxomolybdate catalogue. 3 crystallizes in the triclinic space group P 1 with a =1 22235(1) nm, b =1 52977(2) nm, c =1 54022(1) nm, α =113 746(1)°, β =96 742(1)°, γ = 101 564(1)°, V =2 51892(4) nm 3, Z =1, D c=2 568 g·cm -3 . 4 and 5 crystallize in the monoclinic system: P 2(1)/ n , a =1 08298(2) nm, b =1 54029(1) nm, c = 2 78893(5) nm, β =94 2730(10)°, V =4 63929(12) nm 3, Z =2 and D c=2 671 g·cm -3 for 4, and C 2/ c , a =2 59907(8) nm, b =1 65992(3) nm, c =2 28473(7) nm, β = 93 4370(10)° , V =9 8392(5) nm 3, Z =4 and D c=2 556 g·cm -3 for 5. The structures of 3, 4 and 5 consist of 18 membered “host vip” polyoxoanions [{Na(X) 2}{( μ 3 OH) 4Mo V 8Mo VI 10 O 52 ( μ 2 CH 3COO) 2}] -( n +9) (X=CH 3COO - for 3, DMF for 4 and H 2O for 5), which are connected via Na + ions or hydrogen bonds into infinite extended frameworks.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2009. 272)
文摘A new polyoxomolybdate compound [Ag 3 （HL） 4 ]（PMo 12 O 40）] 1 （HL=3-（2-pyridyl）pyrazole） has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in triclinic,space group P1 with a=10.375（3）,b=12.076（3）,c=13.196（4）,α=84.170（4）,β=71.961（3）,γ=86.326（4）°,V=1563.1（7）3,C 32 H 28 Ag 3 Mo 12 N 12 O 40 P,M r=2726.52,D c=2.897 g/cm 3,μ（MoKα）=3.366 mm 1,F（000）=1284,Z=1,the final R=0.0587 and wR=0.1312 for 4139 observed reflections （I 2σ（Ⅰ））.X-ray diffraction analyses reveal that the PMo 12 O 40 3clusters in compound 1 are linked by four Ag 3 （HL） 4 3＋ units via the terminal oxygen atoms to form a two-dimensional architecture.The symmetrical unit of Ag 3 （HL） 4 3＋ exhibits two distinct Ag（Ⅰ） environments：a two-coordinate {AgN 2 } site and a five-coordinate {AgN 3 O 2 } site which links to two molybdate clusters.
基金supported by the Science and Technology Research Projects of the Education Department of Jilin Province (No. 2009. 272)
文摘A new polyoxomolybdate compound [Zn（HL）2（Mo8O26）（4,4＇-Bipy）]·（4,4＇-Bipy） （HL = 3-（2-pyridyl）pyrazole, 4,4＇-Bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, TG and IR spectroscopy. The compound crystallizes in monoclinic, space group C2/c with a = 18.060（4）, b = 13.870（3）, c = 19.360（4） A, β = 93.50（3）°, V = 4840.5（17） 3, C36H30Mo8N10O26Zn, Mr = 1851.59, Dc = 2.541 g/cm^3, μ（MoKα） = 2.589 mm·1, F（000） = 3560, Z = 4, the final R = 0.0328 and wR = 0.0870 for 4005 observed reflections （I 〉 2σ（I））. X-ray diffraction analyses reveal that compound 1 is constructed from Mo8O264-units linked by Zn（HL）22＋ and 4,4＇-Bipy. Mo8O264-is connected by Zn（HL）2^2＋ via terminal oxygen atoms along the [010] axis forming chains, which are further linked by 4,4＇-Bipy along the [001] axis forming a two-dimensional network structure.
基金This project was supported by the 973 program of the MOST (001CB108906) the National Natural Science Foundation of China (90206040+4 种基金20073048) the NSF of Fujian Province (2002F015 2002J006) the State Key Lab of Chemistry (030065) the Chinese Academy of Sciences
文摘The title compound, {(H3O)4(NH4)4[Mo8O28]?2H2O}n 1, has been synthesized from the reaction of Zn(OAc)2 and (NH4)6Mo7O24?4H2O in aqueous solution at ambient tempe- rature, and its crystal structure was determined by X-ray single-crystal analysis with the following crystallographic data: monoclinic system, space group P21/n, a = 9.5234(6), b = 11.3235(8), c = 14.8812(10) ?, β = 107.467(2)o, V = 1530.77(18) ?3, Z = 4, F(000) = 1336, μ = 3.293 mm-1 and Dc = 3.037 g/cm3. The final R = 0.0619 for 2691 observed reflections (I > 2σ(I)). X-ray crys- tal structure analysis showed that the novel one-dimensional chain compound is built up by basic {Mo8O28} units via single μ2-O, and such chains are further linked into a three-dimensional net- work by hydrogen bonds.
基金support by the Basic Energy Sciences,Department of Energy (DEFG0286ER45237).
文摘Polymeric systems have played an important role as structure-directing agents and in the control of nucleation and growth of crystals.This article reviews the work of our research group in the field of the polymer-assisted crystallization of inorganic materials,mainly focused on the formation of highly ordered,porous molybdenum oxide nanostructures.Different experimental parameters including the influence of poly(ethylene oxide)-containing polymers on the morphology and structure of the products obtained fr...
基金The work was supported by NNSFC (No. 20501011)Liaocheng University (31801)
文摘One new polyoxometalate compound connected via nickel/potassium cations, H8K{[Ni（H2O）5]2（H2Mo1.80W10.20O42）}Cl3·16H2O 1, was prepared and characterized by elemental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis results reveal that clusters of [Ni（H2O）5]2（H2Mo1.80W10.20O42）}^6-in compound 1 are linked by potassium cations to form one- dimiensional chains, based on which a three-dimensional network is further constructed via the hydrogen bonds of O…O and O…Cl. Magnetic measurements show that compound 1 has paramagnetic properties. Crystal data： H62Cl3KMo1.80Ni2O68W10.20, Mr = 3461.33, monoclinic, space group C2/c, a = 18.9291（19）, b = 16.6758（17）, c = 19.1064（19）A, β = 106.6880（10）°, V = 5777.1（10）A^3, Z = 4, Dc = 3.980 g/cm^3, F（000） = 6250, μ = 21.574 mm^-1, R = 0.0579 and wR = 0.1623 （Ⅰ 〉 2σ（Ⅰ））.
基金The project was supported by the National Natural Science Foundation of China (20171012) and the Natural Science Foundation of Fujian Province, China (E0110010).
文摘A novel 3-D inorganic bimetallic compound Ag2Mo2O7 has been hydrothermally synthesized and structurally characterized by X-ray diffraction. The compound crystallizes in monoclinic, space group P21/c with a = 6.1274（3）, b = 13.1836（6）, c = 7.8780（3）A, β= 110.673（3）°, V = 595.42（5）A3, Z= 4, Mr= 519.62, Dc = 5.797g/cm^3, F（000） = 936,μ（MoKα） = 10.579 mm^-1, F（000） = 936, the final R = 0.0204 and wR = 0.0477 for 1268 observed reflections with I〉 2σ（I）. In the title compound, the [Mo4O16]n^8n-chains are linked through O-Ag-O bridging bonds to form a 3D network. It represents an unprecedented linking mode between the isopolyoxomolybdate chain and the transition metal oxide cluster. IR, TGA and fluorescence properties of the title compound are also studied.
